CN103305052A - Nanometer ni-p conductive ink and preparation method thereof - Google Patents
Nanometer ni-p conductive ink and preparation method thereof Download PDFInfo
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- CN103305052A CN103305052A CN2013102460043A CN201310246004A CN103305052A CN 103305052 A CN103305052 A CN 103305052A CN 2013102460043 A CN2013102460043 A CN 2013102460043A CN 201310246004 A CN201310246004 A CN 201310246004A CN 103305052 A CN103305052 A CN 103305052A
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Abstract
The invention discloses a nanometer Ni-P conductive ink and a preparation method thereof, belongs to the field of nanometer materials. The conductive ink comprises one or more of amorphous nano Ni-P powder, water, ethanol and ethylene glycol, one or more of oleic acid, polyethylene glycol and OP-10 emulsifier; the mass content of the amorphous nano Ni-P powder is 10-30%; and the grain size is 30-85 nm. The preparation method orderly comprises the following steps of: preparing nickel salt and sodium hypophosphite into a water solution according to the molar ratio of 0.3; adding the prepared reaction mixing solution into a nucleation revulsant to trigger reaction and disperse; centrifuging, edulcorating and drying the reacted mixing solution to prepare the amorphous nano Ni-P powder; and preparing the conductive ink according to the ratio, wherein the nucleation revulsant is sodium borohydride and/or potassium borohydride. The invention provides the nano Ni-P conductive ink with low price and excellent performance, and the preparation method thereof.
Description
Technical field
The invention belongs to field of nanometer material technology, relate to a kind of conductive ink, especially relate to a kind of nanometer Ni-P conductive ink.
Background technology
In the electronic industry, the problem such as that the conventional lithographic techniques printed circuit board exists is consuming time, expensive, environmental pollution, optional base material are limited, possesses the inkjet technology that does not need to contact, do not have pressure, do not need the advantages such as forme, caused the very big concern of the developed countries such as European Union, the U.S., Japan, and this technology can be widely used in various electronic products, such as printed electronic circuit (PCB and FPC), electronic tag (RFID), Organic Light Emitting Diode (OLED), intelligent display screen, conventional batteries and solar cell, sensor and Electronic Packaging etc.ABC Nanotec Solution of Taejon city, Korea, succeeded in developing a kind of conductive nano ink, be applied to just identify (RFID) electronic tag, printed circuit board (PCB) (PCB), flexible printed circuit board (FPCB) at the intelligent wireless of high speed development, also can be used for printed circuit board (PCB) shielding electromagnetic waves material.This shows, by means of the ink-jet technology of day by day popularizing, conductive ink may become the main raw material that high integrated, high-accuracy pcb board of future generation is produced.
Conductive ink (electrically conductive ink) is a kind of being printed on the various non-conductive stocks, behind the dry also sintering, because the distance of conductive ion key diminishes, unbound electron moves the formation electric current along outer field orientation, have the printing ink of good conduction current and eliminating accumulate static charge ability, can be divided into gold and silver, copper etc. according to conductive filler material.At present, the Japanese industries Technical Integration Studies has been developed a kind of printing ink that contains nanometer-level silver; The U.S. researchist of University of Illinois is loaded on the nanometer silver ink and draws linear array in the ballpoint pen, make be connected to top LED be communicated with luminous, but the price of the type printing ink approximately is 10000 dollars/liter; Domestic also to the development of nano silver conductive ink just probe into, Chen Mingwei, Lv Chunlei, the seal Renhe, Wang Weijiang, Yu Zuzhan " preparation of nano-copper conductive ink and research " has also done correlative study to the preparation of nano-copper conductive ink, and the copper particle that makes 40-50nm has the advantages such as cost is low, anti-ion mobility characteristics.But above research all is that Financial cost is high, becomes the biggest obstacle that industry is promoted with the conductive ink of expensive nano-silver powder, bronze and copper powder preparation, and the very easily oxidation of the active height of copper nanoparticle.
Therefore, exploitation conductive nano ink cheap and excellent performance is the Focal point and difficult point of ink-jet technology research of receiving much concern.
Summary of the invention
The object of the invention is to: nanometer Ni-P conductive ink of a kind of cheap and excellent performance and preparation method thereof is provided.
The object of the invention realizes by following technical proposals:
A kind of nanometer Ni-P conductive ink, comprise amorphous nano Ni-P powder, and in the water, ethanol, ethylene glycol one or more, one or more in oleic acid, polyoxyethylene glycol, the OP-10 emulsifying agent, wherein amorphous nano Ni-P powder quality content 10～30%, and particle diameter is 30-85nm.
In the such scheme, adopt Ni-P powder cost low, resistance to oxidation, wherein creativeness has adopted nickel powder, has good electroconductibility, and non-crystal structure has good solidity to corrosion, conductivity, water, ethanol, ethylene glycol are used for dissolving, disperse the nickel phosphor powder, and oleic acid, polyoxyethylene glycol, OP-10 emulsifying agent are for reducing the reunion of nanometer powder, and certain content Ni-P powder guarantees the printing ink effect, this scheme good dispersity has overcome in the prior art nanometer this difficult problem that is difficult to overcome of reuniting.
Described amorphous nano refers to the nano material of non-crystal structure.
Described OP-10 emulsifying agent, English chemical name: Emulsifier OP-10 forms: the condenses of alkylphenol and oxyethane belongs to nonionic surface active agent.
A kind of preparation method of aforesaid nanometer Ni-P conductive ink may further comprise the steps successively:
(1), 0.3 (be nickel salt: inferior sodium phosphate=0.3) be mixed with mixed aqueous solution in molar ratio with nickel salt and inferior sodium phosphate;
(2), with the reaction mixture for preparing in (1) under 20 ℃～40 ℃ of constant temperature, regulator solution pH to 5～8 add the initiation reaction of forming core inductor and disperse;
(3), reacted mixed solution is centrifugal, removal of impurities, drying, prepare amorphous nano Ni-P powder;
(4), the nanometer Ni-P powder that (3) is prepared is scattered in in water, ethanol, the ethylene glycol one or more, and add in oleic acid, polyoxyethylene glycol, the OP-10 emulsifying agent one or more, the nanometer Ni-P conductive ink of preparation amorphous nano Ni-P powder quality content 10～30%; Wherein, described forming core inductor is sodium borohydride and/or POTASSIUM BOROHYDRIDE.
As optimal way, described forming core inductor add-on is 0.0053～0.0159mol/L.
As optimal way, in described (1) step, nickel salt is single nickel salt and/or nickelous chloride.
As further preferred embodiment, in described (2) step, the pH adjusting agent of regulator solution pH is strong basic reagent.
As further preferred embodiment, described pH adjusting agent is sodium hydroxide and/or potassium hydroxide.
Compared with prior art, beneficial effect of the present invention is:
1. the present invention uses amorphous nano Ni-P power stability can have 20 days at ambient stable well, and is not stratified.
2. nano nickel phosphor powder particle diameter is little, and good dispersity, without obviously reuniting, is uniformly dispersed.
3. cost of the present invention is low, and very high economical and practical value is arranged.
Nanometer Ni-P conductive ink prepare simple, easy to operate, cost is low, produce without bazardous waste.
Description of drawings
Fig. 1 is the AFM X-Y scheme of nano-nickel powder in the nanometer Ni-P conductive ink among the embodiment 1;
Fig. 2 is the XRD figure of amorphous nano nickel powder in the nanometer Ni-P conductive ink among the embodiment 1;
Fig. 3 is the AFM X-Y scheme of nano-nickel powder in the nanometer Ni-P conductive ink among the embodiment 2;
Fig. 4 is the particle size analysis figure of nano-nickel powder in the nanometer Ni-P conductive ink among the embodiment 2;
Fig. 5 is the XRD figure of amorphous nano nickel powder in the nanometer Ni-P conductive ink among the embodiment 2;
Fig. 6 is nano-nickel powder AFM X-Y scheme in the nanometer Ni-P conductive ink among the embodiment 3;
Fig. 7 is the particle size analysis figure of nano-nickel powder in the nanometer Ni-P conductive ink among the embodiment 3;
Fig. 8 is the AFM X-Y scheme of nano-nickel powder in the nanometer Ni-P conductive ink among the embodiment 4;
Fig. 9 is the AFM three-dimensional plot of nano-nickel powder in the nanometer Ni-P conductive ink among the embodiment 4;
Figure 10 is the particle size analysis figure of nano-nickel powder in the nanometer Ni-P conductive ink among the embodiment 4;
Figure 11 is the XRD figure of amorphous nano nickel powder in the nanometer Ni-P conductive ink among the embodiment 4.
Embodiment
Following non-limiting examples is used for explanation the present invention.
Embodiment 1:
6.5375g nickel sulfate hexahydrate and 7.5g inferior sodium phosphate are dissolved in respectively in the 50ml deionized water, stir, after mixing 250ml volumetric flask constant volume, the cooling, 20 ℃ of insulations add 4 milliliters of 1mol/L sodium hydroxide solutions and regulate pH; Slowly add 0.025g sodium borohydride, 0.033g hydrazine hydrate, 0.1429g POTASSIUM BOROHYDRIDE, continue to stir 60 minutes, be cooled to room temperature, ageing 6 hours obtains Ni-P nano-nickel powder dispersion liquid; With the dispersion liquid that obtains under 6000 rev/mins rotating speed centrifugal 30 minutes, use respectively ammoniacal liquor, deionized water and absolute ethanol washing twice, then at room temperature vacuum-drying is 3 hours, obtains the Ni-P nano-nickel powder; Take by weighing the 0.2g nano-nickel powder, be dissolved in the 0.5g ethylene glycol solvent, and add 0.3g dispersion agent-polyoxyethylene glycol, obtain 20% nanometer Ni-P conductive ink.
With Ni-P nano-nickel powder sampling obtained above, use X-ray diffractometer (XRD) that it is carried out the phase atlas analysis, such as Fig. 2, judge that this product is nickel phosphorus mixed crystal powder.To the sampling of Ni-P conductive ink, use atomic force microscope (AFM) to observe nano-nickel powder in the nanometer Ni-P conductive ink, as can be seen from Figure 1, the Ni-P powder is spherical in the conductive ink, particle diameter is that particle is intensive about 85nm, disperses comparatively even; This product room temperature sealing place 7 days not stratified.
Embodiment 2:
3.2234g nickelous chloride and 7.5g inferior sodium phosphate are dissolved in respectively in the 50ml deionized water, stir, after mixing 250ml volumetric flask constant volume, the cooling, 40 ℃ of insulations add 4 milliliters of 1mol/L sodium hydroxide solutions and regulate pH; Slowly add the 0.066g hydrazine hydrate, continue to stir 40 minutes, be cooled to room temperature, ageing 6 hours obtains Ni-P nano-nickel powder dispersion liquid; With the dispersion liquid that obtains under 6000 rev/mins rotating speed centrifugal 30 minutes, use respectively ammoniacal liquor, deionized water and absolute ethanol washing twice, then at room temperature vacuum-drying is 3 hours, obtains the Ni-P nano-nickel powder; Take by weighing the 0.3g nano-nickel powder, be dissolved in the 0.6g ethylene glycol solvent, and add 0.1g dispersion agent oleic acid, obtain 30% nanometer Ni-P conductive ink.
With Ni-P nano-nickel powder sampling obtained above, use X-ray diffractometer (XRD) that it is carried out the phase atlas analysis, obtain result such as Fig. 5.To the sampling of Ni-P conductive ink, use atomic force microscope (AFM) to observe nano-nickel powder in the nanometer Ni-P conductive ink, result such as Fig. 3,4, the Ni-P powder is spherical in the conductive ink, and particle diameter is about 30nm, and the particle dispersion effect is fine, without reuniting, the room temperature sealing deposit 7 days not stratified.
Embodiment 3:
3.2686g nickel sulfate hexahydrate, 1.6117g nickelous chloride and 7.5g inferior sodium phosphate are dissolved in respectively in the 50ml deionized water, stir, after mixing 250ml volumetric flask constant volume, cooling, be transferred to beaker and be heated to 40 ℃, add 4 milliliters of 1mol/L sodium hydroxide solutions and regulate pH; Slowly add the 0.066g hydrazine hydrate, continue to stir 60 minutes, be cooled to room temperature, ageing 6 hours obtains Ni-P nano-nickel powder dispersion liquid; With the dispersion liquid that obtains under 8000 rev/mins rotating speed centrifugal 15 minutes, use respectively ammoniacal liquor, deionized water and absolute ethanol washing twice, then at room temperature vacuum-drying is 3 hours, obtains the Ni-P nano-nickel powder; Take by weighing the 0.3g nano-nickel powder, be dissolved in the 0.5g alcohol solvent, and add the 0.2gOP-10 emulsifying agent, obtain 30% nanometer Ni-P conductive ink.
To the sampling of Ni-P conductive ink, use atomic force microscope (AFM) to observe nano-nickel powder in the nanometer Ni-P conductive ink, result such as Fig. 6,7, the Ni-P powder is spherical in the conductive ink, particle diameter is 56.71nm, is uniformly dispersed, without obviously reuniting; Room temperature sealing deposit 10 days not stratified.
Embodiment 4:
3.2234g nickelous chloride and 7.5g inferior sodium phosphate are dissolved in respectively in the 50ml deionized water, stir, after mixing 250ml volumetric flask constant volume, the cooling, be transferred to beaker and be heated to 40 ℃, add 4 milliliters of 1mol/L sodium hydroxide solutions and regulate pH; Slowly add the 0.857g POTASSIUM BOROHYDRIDE, continue to stir 40 minutes, be cooled to room temperature, ageing 6 hours obtains Ni-P nano-nickel powder dispersion liquid; With the dispersion liquid that obtains under 8000 rev/mins rotating speed centrifugal 15 minutes, use respectively ammoniacal liquor, deionized water and absolute ethanol washing twice, then at room temperature vacuum-drying is 3 hours, obtains the Ni-P nano-nickel powder; Take by weighing the 0.1g nano-nickel powder, be dissolved in 0.3g ethylene glycol, 0.2g ethanol, 0.1g distilled water mixed solution, and add 0.1g dispersion agent oleic acid, 0.1g Polyethylene Glycol-600,0.1gOP-10 emulsifying agent, obtain 10% nanometer Ni-P conductive ink.
With Ni-P nano-nickel powder sampling obtained above, use X-ray diffractometer (XRD) that it is carried out the phase atlas analysis, and compare with without phosphorus nickel powder, judge that this product is non-crystal structure, the result as shown in figure 11, (a) is the nano nickel phosphor powder among the figure, (b) self-control nickel powder.To the sampling of Ni-P conductive ink, use atomic force microscope (AFM) to observe nano-nickel powder in the nanometer Ni-P conductive ink, result such as Fig. 8,9,10, the Ni-P powder is spherical in the conductive ink, particle diameter is 80.60nm, is uniformly dispersed, without obviously reuniting; Room temperature sealing deposit 10 days not stratified.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. nanometer Ni-P conductive ink, it is characterized in that: comprise amorphous nano Ni-P powder, and in the water, ethanol, ethylene glycol one or more, in oleic acid, polyoxyethylene glycol, the OP-10 emulsifying agent one or more, wherein amorphous nano Ni-P powder quality content 10～30%, and particle diameter is 30-85nm.
2. nanometer Ni-P conductive ink as claimed in claim 1 is characterized in that: described amorphous nano Ni-P powder is for spherical.
3. the preparation method of a claim 1 or 2 described nanometer Ni-P conductive inks is characterized in that may further comprise the steps successively:
(1), nickel salt and inferior sodium phosphate 0.3 are mixed with mixed aqueous solution in molar ratio;
(2), with the reaction mixture for preparing in (1) under 20 ℃～40 ℃ of constant temperature, regulator solution pH to 5～8 add the initiation reaction of forming core inductor and disperse;
(3), reacted mixed solution is centrifugal, removal of impurities, drying, prepare amorphous nano Ni-P powder;
(4), the nanometer Ni-P powder that (3) is prepared is scattered in in water, ethanol, the ethylene glycol one or more, and add in oleic acid, polyoxyethylene glycol, the OP-10 emulsifying agent one or more, the nanometer Ni-P conductive ink of preparation amorphous nano Ni-P powder quality content 10～30%; Wherein, described forming core inductor is sodium borohydride and/or POTASSIUM BOROHYDRIDE.
4. the preparation method of nanometer Ni-P conductive ink as claimed in claim 3 is characterized in that: in described (1) step, nickel salt is single nickel salt and/or nickelous chloride.
5. the preparation method of nanometer Ni-P conductive ink as claimed in claim 3, it is characterized in that: described forming core inductor add-on is 0.0053～0.0159mol/L.
6. such as the preparation method of claim 3,4 or 5 described nanometer Ni-P conductive inks, it is characterized in that: in described (2) step, the pH adjusting agent of regulator solution pH is strong basic reagent.
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| CN108384406A (en) * | 2018-05-29 | 2018-08-10 | 四川理工学院 | A kind of graphene oxide UV is coating material solidified and preparation method thereof |
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| JP2007173075A (en) * | 2005-12-22 | 2007-07-05 | Sekisui Chem Co Ltd | Conductive particulate and anisotropic conductive material |
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| JP2007173075A (en) * | 2005-12-22 | 2007-07-05 | Sekisui Chem Co Ltd | Conductive particulate and anisotropic conductive material |
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| 沈俭一等: ""诱导自催化法制备Ni-P超细非晶合金的动力学研究"", 《化学学报》 * |
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| CN108384406A (en) * | 2018-05-29 | 2018-08-10 | 四川理工学院 | A kind of graphene oxide UV is coating material solidified and preparation method thereof |
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